CN107247080B - On-line detection system for oxygen ions in high-temperature molten salt - Google Patents
On-line detection system for oxygen ions in high-temperature molten salt Download PDFInfo
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Abstract
The invention belongs to the field of electrochemical analysis and test of high-temperature molten salt, and provides an online detection system for detecting oxygen ions in the high-temperature molten salt, which comprises: the device comprises a zirconium oxide electrode, a reference electrode, a thermocouple, a temperature recorder, an electrochemical workstation, a computer, a fixing device and a signal wire; the zirconia electrode, the reference electrode and the thermocouple are fixed on the fixing device through the lower electrode fixing piece; the zirconia electrode and the reference electrode are connected with the electrochemical workstation through signal wires; the thermocouple is connected with the temperature recorder through a signal wire; the electrochemical workstation and the temperature recorder are connected with a computer. The detection system has the advantages of simple structure, convenience in assembly, small volume and light weight, is suitable for the concentration of oxygen ions in high-temperature molten salt with various components, realizes online detection, and is very suitable for laboratories.
Description
Technical Field
The invention belongs to the field of high-temperature molten salt electrochemical analysis and test, and particularly relates to an on-line detection system for oxygen ions in high-temperature molten salt.
Background
High temperature molten salts are commonly used as chemical reaction media in the metallurgical industry due to their advantages of good electrical conductivity, low steam pressure, low viscosity, and large thermal capacity. With the rapid development of molten salt metallurgy, the molten salt metallurgy process has higher requirements on the quality of molten salt, wherein the concentration of oxygen ions in the molten salt is an important factor of the properties of the molten salt, and the influence on the molten salt metallurgy process is great. Therefore, it is very important to accurately measure the concentration of dissolved oxygen ions in the molten salt.
At present, no unified and universal measuring method exists for measuring the oxygen content in the molten salt. The oxygen content in the molten salt is partially determined by adopting an oxygen analyzer (inert gas melting infrared spectroscopy), but the oxygen ion content in the molten salt cannot be reflected in real time by adopting the method, and the prediction is difficult; the content of oxygen ions in the molten salt can be measured at a lower concentration by using square wave voltammetry, but the error is larger due to corrosion of a metal anode. The acid-base titration method can analyze the oxygen ion content in the molten salt off line, but the error is larger at lower concentration.
Usually, zirconia is doped with some oxides as a stabilizer, and the sintered and molded yttrium-stabilized zirconia material has better oxygen ion selectivity. Oxygen gasThe yttria-stabilized zirconia solid electrolyte has selectivity to oxygen ions due to the existence of oxygen ion vacancies. When oxygen ion concentration difference exists between the inner side and the outer side of the zirconia electrode, oxygen ion concentration difference potential is generated. The concentration of oxygen ions in the internal reference molten salt in the yttria-stabilized zirconia electrode is kept constant, and when the concentration of oxygen ions in the molten salt to be detected is changed, the concentration difference potential of the oxygen ions at the inner side and the outer side of the electrode is also changed. The oxygen ion concentration in the molten salt can be determined through the corresponding relation between the measured potential and different oxygen ion concentrations. At present, Mn/MnO is used as a measuring element for industrially measuring the oxygen concentration in high-temperature liquid metal2、Cr/Cr2O3、Bi/Bi2O3The electrode is a zirconia electrode used as an internal reference, but the electrodes have a small oxygen concentration measurement range and a large volume, and are not convenient for laboratory online detection of the concentration of oxygen ions in a small amount of high-temperature molten salt.
Disclosure of Invention
Objects of the invention
In order to overcome the defects of the prior art, the invention provides the on-line detection system which has the advantages of small volume, simple structure, large measuring range, accurate measurement and suitability for on-line detection of a small amount of oxygen ions in high-temperature molten salt in a laboratory.
(II) technical scheme
In order to solve the defects of the prior art, the invention is realized by the following scheme:
an on-line detection system for oxygen ions in high temperature molten salts, the on-line detection system comprising: the device comprises a zirconium oxide electrode, a reference electrode, a thermocouple, a temperature recorder, an electrochemical workstation, a computer and a fixing device; the zirconia electrode, the reference electrode and the thermocouple are fixed on the fixing device through the lower electrode fixing piece; the zirconia electrode and the reference electrode are connected with an electrochemical workstation; the thermocouple is connected with a temperature recorder; the electrochemical workstation and the temperature recorder are connected with a computer.
The zirconia electrode mainly comprises: upper electrode mounting, electrode fixing ball, lower electrode mounting, electrode main part.
The upper electrode fixing piece is of a screw-shaped structure, a through round hole is formed in the upper electrode fixing piece, and a spherical groove is formed in the lower end face of the upper electrode fixing piece; the lower electrode fixing piece is of a male-female screw-shaped structure, the lower electrode fixing piece is provided with a through round hole, and the bottom of the female threaded hole at the top end is provided with a spherical groove; the upper electrode fixing piece is fixedly connected with the lower electrode fixing piece; the electrode fixing ball is provided with a round hole penetrating through the center of the ball, the diameter of the round hole is the same as the outer diameter of the corundum tube, and the electrode fixing ball is positioned in the spherical grooves of the upper electrode fixing piece and the lower electrode fixing piece.
The electrode main body mainly includes: the device comprises a silver electrode lead, an upper sealing plug, a corundum tube, a lower sealing plug, a zirconia tube and internal reference molten salt; the upper sealing plug is provided with a through circular hole, the upper sealing plug is fixedly connected with the upper end of the corundum tube, and the fixed connection part of the upper sealing plug and the corundum tube is sealed; the corundum tube penetrates through the upper electrode fixing piece, the electrode fixing ball and the lower electrode fixing piece; the lower sealing plug is provided with a through round hole, the lower sealing plug is fixedly connected with the upper end of the zirconia tube, and the joint of the lower sealing plug and the zirconia tube is sealed; the zirconia tube is doped with 8% mol of yttria, the lower end of the zirconia tube is sealed, the upper end of the zirconia tube is fixedly connected with the lower end of the corundum tube, and the joint of the zirconia tube and the corundum tube is sealed; the internal reference molten salt is positioned inside the zirconium oxide tube; the silver electrode lead penetrates through the upper sealing plug, the corundum tube, the lower sealing plug and the zirconia tube, the lower end of the silver electrode lead is immersed into the internal reference molten salt to reach the bottom of the zirconia tube, and the upper end of the silver electrode lead extends out of the upper sealing plug.
The internal reference molten salt is AgCl-containing and extremely small amount of Li2CO3The measured high-temperature molten salt has AgCl content of 0.5-0.8mol/kg and Li2CO3The content is 0.03-0.1mol/kg, and the addition amount of the internal reference ratio molten salt is 0.5-1 g.
The thickness of the zirconia tube is 1-2 mm.
The fixed connection part of the upper sealing plug and the corundum tube is formed by winding the upper sealing plug by adopting a polytetrafluoroethylene raw material belt and coating the polytetrafluoroethylene raw material belt with high-temperature ceramic glue for sealing.
The fixed connection part of the lower sealing plug and the zirconia tube is sealed by high-temperature ceramic glue.
The zirconia tube is fixedly connected with the corundum tube in an adhesive manner.
The upper sealing plug and the lower sealing plug are made of high-temperature resistant materials.
The electrode fixing ball is made of an elastic material.
(III) advantageous effects
In order to overcome the problem of insufficient online detection means for oxygen ions in high-temperature molten salt in the prior art, the invention designs and develops an online detection system for oxygen ions in high-temperature molten salt, wherein on the basis of the corresponding relation between the potential difference of a zirconia electrode and a reference electrode and the concentration of the oxygen ions, the detection of the oxygen ions is converted into potential difference monitoring, and temperature data is introduced to correct the corresponding relation between the potential difference and the concentration of the oxygen ions, so that the detection accuracy of the oxygen ions is greatly improved, and the online detection of the concentration of the oxygen ions in the high-temperature molten salt is realized by matching with the zirconia electrode.
In order to solve the problems of large volume, small measurement range, poor accuracy and the like of the measurement equipment in the prior art, the invention provides a zirconium oxide electrode. The zirconia electrode only comprises a main body electrode, an upper electrode fixing piece, an electrode fixing ball and a lower electrode fixing piece, so that the electrode is simple in structure, convenient to assemble, small in size, light in weight, suitable for the concentration of oxygen ions in high-temperature molten salt with various components, and very suitable for being used in a laboratory; the electrode fixing ball is extruded towards the middle when the upper electrode fixing part and the lower electrode fixing part are screwed up by combining the matching of the upper electrode fixing part, the electrode fixing ball and the lower electrode fixing part, and the corundum tube is extruded towards the middle when the electrode fixing ball is extruded, so that the aim of fixing the zirconia electrode is fulfilled; the zirconia electrode is formed by doping 8% yttria, has a thickness of 1-2mm, and contains AgCl with a content of 0.5-0.8mol/kg and Li2CO30.5-1g of high-temperature molten salt with the content of 0.03-0.1mol/kg, and greatly increases the sensitivity and range of oxygen ion detection.
Drawings
Fig. 1 is a schematic view of the structure of a zirconia electrode.
FIG. 2 is a diagram of the main components of a zirconia electrode.
FIG. 3 is a schematic diagram of online detection of oxygen ion concentration in high-temperature molten salt.
FIG. 4 is an electromotive force variation curve of a device for online detection of the concentration of oxygen ions in molten salt during calibration.
Wherein 1 silver electrode lead 2, upper sealing plug 3, upper electrode fixing part 4, electrode fixing ball 5, lower electrode fixing part 6, corundum tube 7, lower sealing plug 8, zirconia tube 9, reference molten salt 10, electrode body 11, zirconia electrode 12, reference electrode 13, thermocouple 14, temperature recorder 15, electrochemical workstation 16, computer 17, fixing device 18, signal wire 19, molten salt to be tested
Detailed Description
The invention is described in further detail in the following detailed description with reference to the accompanying drawings:
as shown in fig. 3, the system includes: a zirconia electrode 11, a reference electrode 12, a thermocouple 13, a temperature recorder 14, an electrochemical workstation 15, a computer 16 and a fixing device 17; the zirconia electrode 11, the reference electrode 12 and the thermocouple 13 are fixed on a fixing device 17 through a lower electrode fixing piece 5; the zirconia electrode 11 and the reference electrode 12 are connected with an electrochemical workstation 15; the thermocouple 13 is connected with a temperature recorder 14; the electrochemical workstation 15 and the temperature recorder 14 are connected with a computer 16.
As shown in fig. 2, the zirconia electrode 11 mainly includes: an upper electrode fixing member 3, an electrode fixing ball 4, a lower electrode fixing member 5, and an electrode main body 10; the upper electrode fixing piece 3 is of a screw-shaped structure, the upper electrode fixing piece 3 is provided with a through round hole, and the lower end face of the upper electrode fixing piece is provided with a spherical groove; the lower electrode fixing piece 5 is of a male-female screw-shaped structure, the lower electrode fixing piece 5 is provided with a through round hole, and the bottom of a female threaded hole at the top end is provided with a spherical groove; the upper electrode fixing piece 3 is in threaded connection with the lower electrode fixing piece 5; the electrode fixing ball 4 is provided with a round hole penetrating through the center of the ball, the diameter of the round hole is the same as the outer diameter of the corundum tube 6, and the electrode fixing ball 4 is positioned in the spherical grooves of the upper electrode fixing part 3 and the lower electrode fixing part 5;
as shown in fig. 1, the electrode main body 10 mainly includes: the device comprises a silver electrode lead 1, an upper sealing plug 2, a corundum tube 6, a lower sealing plug 7, a zirconia tube 8 and internal reference molten salt 9; the upper sealing plug 2 is provided with a through round hole made of polytetrafluoroethylene; a polytetrafluoroethylene raw material tape is wound outside the upper sealing plug 2, and high-temperature ceramic glue is coated on the surface of the polytetrafluoroethylene raw material tape and used for blocking the upper port of the corundum tube 6; the upper electrode fixing part 3, the electrode fixing ball 4 and the lower electrode fixing part 5 are sleeved on the corundum tube 6; the lower sealing plug 7 is provided with a through round hole made of quartz; a polytetrafluoroethylene raw material tape is wound outside the lower sealing plug 7, and high-temperature ceramic glue is coated on the surface of the polytetrafluoroethylene raw material tape and used for blocking the upper port of the zirconia tube 8; 8% mol of yttrium oxide is doped in the zirconia tube 8, and the lower end of the zirconia tube 8 is sealed; the upper end of the zirconia tube 8 is bonded with the lower end of the corundum tube 6; the internal reference molten salt 9 is positioned at the bottom of the zirconia tube 8; the silver electrode lead 1 penetrates through the upper sealing plug 2, the corundum tube 6, the lower sealing plug 7 and the zirconia tube 8, the lower end of the silver electrode lead is immersed into the internal reference molten salt 9 to the bottom of the zirconia tube 9, and the upper end of the silver electrode lead extends out of the upper sealing plug 2.
When the upper end machine fixing part 3 and the lower electrode fixing part 5 are screwed up, the electrode fixing ball 4 positioned in the spherical groove is extruded towards the middle, so that the electrode fixing ball 4 is forced to extrude the corundum tube 6 positioned in the circular hole through which the electrode fixing ball 4 penetrates towards the middle, and the effect of fixing the zirconia electrode is realized.
And (3) assembling the zirconia electrode 11 and the detection system according to the structural relationship, placing the zirconia electrode 11, the reference electrode 12 and the thermocouple 13 in the high-temperature molten salt to be measured, and starting the temperature recorder 14, the electrochemical workstation 15 and the computer 16 to measure.
Example 1
The operation steps are as shown above, and only the structural parameters are different, and the specific parameters are as follows: the size of the zirconia tube is 6mm, the wall thickness is 1mm, and the length is 150 mm; the internal reference molten salt is eutectic salt powder of lithium chloride and potassium chloride with the mass of 1g, wherein the eutectic salt powder comprises 0.75mol/kg of silver chloride and 0.03mol/kg of lithium carbonate; the temperature of the high-temperature molten salt is 500 ℃.
Inserting a zirconia oxygen electrode into lithium chloride and potassium chloride molten salt at 500 ℃, introducing hydrogen chloride gas into the molten salt, and rapidly increasing the electromotive force of the zirconia electrode to re-stabilize the zirconia electrode within 400 s; stopping introducing hydrogen chloride gas after a period of stabilization, starting introducing argon gas, removing hydrogen chloride in the molten salt through bubbling, and starting to reduce the potential of the electrode; after the electromotive force is stabilized, adding lithium carbonate into the molten salt, rapidly reducing the electromotive force and achieving the stabilization within 400S. Repeating the above operation 3 times in the molten salt, wherein the measured potential changes the same each time, and FIG. 4 shows the electrode potential of the above zirconia oxygen ion measuring electrode in the process of repeatedly introducing hydrogen chloride gas and argon gas, and the measured oxygen ion concentration in the high temperature molten salt is 5 ppm. From fig. 4, it can be known that the oxygen ion detection system is sensitive to the oxygen ion concentration in the molten salt, and the measurement reproducibility of the oxygen ion detection system under the same condition is good.
Example 2
The operation is the same as in example 1, except that: the size of the zirconia tube is 6mm, the wall thickness is 2mm, and the length is 150 mm; the internal reference ratio molten salt is eutectic salt powder of lithium chloride and potassium chloride of 0.4mol/kg silver chloride and 0.03mol/kg lithium carbonate, and the mass is 0.5 g; the temperature of the high-temperature molten salt is 575 ℃.
The zirconia electrode is inserted into the sodium chloride and calcium chloride fused salt at 575 ℃. And adding lithium carbonate into the molten salt, rapidly reducing the electromotive force, introducing hydrogen chloride gas into the molten salt after the molten salt is stabilized, rapidly increasing the electromotive force of the zirconia oxygen electrode, stabilizing within 400s, and measuring that the oxygen ion concentration in the high-temperature molten salt is 6 ppm.
Example 3
The same as in working example 1, except that: the size of the zirconia tube is 6mm, the wall thickness is 1mm, and the length is 150 mm; the internal reference ratio molten salt is eutectic salt powder of lithium chloride and potassium chloride of 0.8mol/kg silver chloride and 0.1mol/kg lithium carbonate, and the mass is 0.75 g; the temperature of the high-temperature molten salt is 575 ℃.
The zirconia electrode was inserted into a 400 ℃ lithium chloride, potassium chloride molten salt. And adding lithium carbonate into the molten salt, rapidly reducing the electromotive force, introducing hydrogen chloride gas into the molten salt after the molten salt is stabilized, rapidly increasing the electromotive force of the zirconia oxygen electrode, stabilizing within 400s, and measuring that the oxygen ion concentration in the high-temperature molten salt is 4 ppm.
Claims (8)
1. An on-line detection system for oxygen ions in high-temperature molten salt is characterized in that,
the online detection system comprises: the device comprises a zirconium oxide electrode (11), a reference electrode (12), a thermocouple (13), a temperature recorder (14), an electrochemical workstation (15), a computer (16) and a fixing device (17); the zirconia electrode (11), the reference electrode (12) and the thermocouple (13) are fixed on a fixing device (17) through a lower electrode fixing piece (5); the zirconia electrode (11) and the reference electrode (12) are connected with an electrochemical workstation (15); the thermocouple (13) is connected with a temperature recorder (14); the electrochemical workstation (15) and the temperature recorder (14) are connected with the computer (16); the zirconia electrode (11) is internally provided with internal reference molten salt (9);
the zirconia electrode (11) further comprises: an upper electrode fixing part (3), an electrode fixing ball (4), a lower electrode fixing part (5) and an electrode main body (10);
the upper electrode fixing piece (3) is of a screw-shaped structure, a through round hole is formed in the upper electrode fixing piece (3), and a spherical groove is formed in the lower end face of the upper electrode fixing piece; the lower electrode fixing piece (5) is of a male-female screw-shaped structure, a through round hole is formed in the lower electrode fixing piece (5), and a spherical groove is formed in the bottom of the female screw hole in the top end; the upper electrode fixing part (3) is fixedly connected with the lower electrode fixing part (5); the electrode fixing ball (4) is provided with a round hole penetrating through the center of the ball, the diameter of the round hole is the same as the outer diameter of the corundum tube (6), and the electrode fixing ball (4) is positioned in the spherical grooves of the upper electrode fixing piece (3) and the lower electrode fixing piece (5);
the electrode body (10) further comprises: the device comprises a silver electrode lead (1), an upper sealing plug (2), a corundum tube (6), a lower sealing plug (7) and a zirconia tube (8); the upper sealing plug (2) is provided with a through round hole, the upper sealing plug (2) is fixedly connected with the upper end of the corundum tube (6), and the fixed connection part of the upper sealing plug (2) and the corundum tube (6) is sealed; the corundum tube (6) penetrates through the upper electrode fixing piece (3), the electrode fixing ball (4) and the lower electrode fixing piece (5); the lower sealing plug (7) is provided with a through round hole, the lower sealing plug (7) is fixedly connected with the upper end of the zirconia tube (8), and the joint of the lower sealing plug (7) and the zirconia tube (8) is sealed; the zirconia tube (8) is doped with 8% mol of yttria, the lower end of the zirconia tube (8) is sealed, the upper end of the zirconia tube (8) is fixedly connected with the lower end of the corundum tube (6), and the joint of the zirconia tube (8) and the corundum tube (6) is sealed; the internal reference molten salt (9) is positioned inside the zirconia tube (8); the silver electrode lead (1) penetrates through the upper sealing plug (2), the corundum tube (6), the lower sealing plug (7) and the zirconia tube (8), the lower end of the silver electrode lead is immersed into the internal reference molten salt (9) to the bottom of the zirconia tube (8), and the upper end of the silver electrode lead extends out of the upper sealing plug (2).
2. The on-line detection system for oxygen ions in high-temperature molten salt according to claim 1, characterized in that the internal reference molten salt (9) contains AgCl and a very small amount of Li2CO3The measured high-temperature molten salt has AgCl content of 0.5-0.8mol/kg and Li2CO3The content is 0.03-0.1mol/kg, and the addition amount of the internal reference ratio molten salt is 0.5-1 g.
3. An on-line detection system for oxygen ions in high temperature molten salt according to claim 1, characterized in that the zirconia tube (8) is 1-2mm thick.
4. The on-line detection system for the oxygen ions in the high-temperature molten salt according to claim 1, wherein the fixed connection position of the upper sealing plug (2) and the corundum tube (6) is formed by winding the upper sealing plug (2) by using a polytetrafluoroethylene raw material tape and coating the polytetrafluoroethylene raw material tape with high-temperature ceramic glue on the surface of the polytetrafluoroethylene raw material tape for sealing.
5. The on-line detection system for the oxygen ions in the high-temperature molten salt according to claim 1, wherein the fixed joint of the lower sealing plug (7) and the zirconia tube (8) is sealed by high-temperature ceramic glue.
6. The on-line detection system for the oxygen ions in the high-temperature molten salt according to claim 1, wherein the zirconia tube (8) and the corundum tube (6) are fixedly connected in a bonding manner.
7. The on-line detection system for the oxygen ions in the high-temperature molten salt according to claim 1, wherein the upper sealing plug (2) and the lower sealing plug (7) are made of high-temperature resistant materials.
8. The on-line detection system for oxygen ions in high-temperature molten salt according to claim 1, characterized in that the electrode fixing ball (4) is made of an elastic material.
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| CN109682870B (en) * | 2019-01-09 | 2021-03-09 | 中国原子能科学研究院 | Method and device for measuring concentration of metal ions in molten salt |
| CN113311046B (en) * | 2021-05-14 | 2023-05-23 | 武汉大学 | Electrochemical device and electrochemical method for measuring concentration of molten salt oxygen anions |
| CN114414644B (en) * | 2022-01-10 | 2023-08-18 | 中国原子能科学研究院 | System and method for measuring oxygen content in liquid alkali metal |
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